CN109613133B - Method for measuring extractable rate of each fraction of residual oil in crude oil - Google Patents
Method for measuring extractable rate of each fraction of residual oil in crude oil Download PDFInfo
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- CN109613133B CN109613133B CN201811554632.7A CN201811554632A CN109613133B CN 109613133 B CN109613133 B CN 109613133B CN 201811554632 A CN201811554632 A CN 201811554632A CN 109613133 B CN109613133 B CN 109613133B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G7/00—Distillation of hydrocarbon oils
- C10G7/12—Controlling or regulating
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/02—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material
- G01N11/04—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture
- G01N11/06—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture by timing the outflow of a known quantity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/14—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
Abstract
The invention provides a method for measuring the extractable rate of each fraction of residual oil in crude oil. The technical scheme is as follows: the method comprises the following steps: a. subjecting the crude oil to true boiling point distillation: a1, atmospheric distillation: a2, distilling under reduced pressure; b. and (3) performing high-temperature simulated distillation on the residual oil after the distillation, b1, determining the Engler viscosity of the residual oil to be measured, b2 and chromatographic determination. The method comprises the steps of distilling crude oil at a real boiling point, heating and melting residual oil in a kettle after distillation, uniformly stirring, dissolving with carbon tetrachloride or carbon disulfide, and analyzing by using a high-temperature simulated distillation liquid chromatogram to obtain a residual oil distillation report and a residual oil quality yield report; the extractable rate of each fraction in the residual oil is obtained, the degree of coincidence with the device data is checked, the utilization efficiency of the crude oil is determined, the process adjustment, the product yield measurement and calculation and the economic benefit measurement and calculation of the oil refining production are guided, and the economic benefit is improved.
Description
Technical Field
The invention relates to a method and a device for testing residual oil refined from crude oil, in particular to a method for measuring the extractable rate of each fraction of the residual oil in the crude oil.
Background
In recent years, the atmospheric and vacuum distillation device in China has the trends of large scale, diversified crude oil processing varieties, intelligentized production operation and the like, and the technical level is greatly improved. As a 'faucet' of an oil refining enterprise, the technical level of an atmospheric and vacuum distillation device is high and low, which not only relates to the effective utilization of crude oil, but also has great influence on the quality, the product yield and the economic benefit of the whole plant, so that the advanced and applicable technology is required to be actively applied, the progress of the atmospheric and vacuum distillation technology is continuously promoted, and the continuous improvement of the whole oil refining level is promoted.
Compared with the international advanced level, the atmospheric and vacuum distillation device in China still has a large gap, mainly has small device scale, low operation load, short operation period, laggard key process technology, high energy consumption and the like. Therefore, the method can be used for determining the extraction rate of each fraction in the residual oil, checking the degree of coincidence with device data, determining the utilization efficiency of the crude oil, and having great guidance on production process adjustment, product yield measurement and economic benefit measurement.
Disclosure of Invention
The invention aims to provide a method for measuring the extractable rate of each fraction of residual oil in crude oil, which aims at overcoming the defects in the prior art, determines the utilization efficiency of the crude oil, is used for guiding the process adjustment of oil refining production, the product yield measurement and calculation, and the economic benefit measurement and calculation, and improves the economic benefit.
The invention provides a method for measuring the extractable rate of each fraction of residual oil in crude oil, which adopts the technical scheme that: the method comprises the following steps:
a. subjecting the crude oil to true boiling point distillation:
a1, atmospheric distillation:
1, weighing a sample and recording the total amount before weighing and the weight after weighing;
2, carrying out normal pressure distillation;
3 when the temperature is reduced to below 100 ℃, closing the instrument;
a2, vacuum distillation
1 weighing the residual oil product after atmospheric distillation and the quality data of a distillation flask, and starting reduced pressure distillation;
2 when the temperature is reduced to below 100 ℃, closing the instrument;
3, pouring out residual oil in the reaction kettle when the instrument is hot after the instrument is closed;
b. the residual oil left after distillation is subjected to high-temperature simulated distillation
b1, determination of Engler viscosity of residual oil to be measured
Heating and melting to-be-detected residual oil, uniformly stirring, measuring the Engler viscosity E100 at 100 ℃, and dissolving with carbon tetrachloride if the E100 is less than or equal to 100, or dissolving with carbon disulfide if the E100 is greater than 100;
b2, chromatography
1 heating and dissolving residual oil with measured Engler viscosity, uniformly stirring, taking a sample bottle, weighing 0.3 g of sample and 2.0 g of carbon disulfide or carbon tetrachloride, recording specific numerical values, and covering a bottle cover in time;
2, putting the corresponding serial numbers of the sample bottles, opening a computer, editing the sequence and starting to run;
and 3, after the sequence operation is completed, checking a distillation report and a quality yield report of each fraction of the residual oil by controlling a chromatograph.
Preferably, the atmospheric distillation in step a1 of the present invention specifically comprises the following steps:
(1) weighing the sample and recording the total amount before weighing and the weight after weighing;
(2) after the sample is weighed, the distillation kettle is placed on a heating device, the position is adjusted to enable the distillation kettle to be tightly connected with the distillation tower, then a pressure display valve is connected, a water-cooling cooler is connected, and a clamp is used for clamping to enable the contact part to be more sealed;
(3) starting the computer, and connecting an instrument to check whether the instrument is normally connected;
(4) the upper heating sleeve turns on the stirring switch to turn on the designated switch, and the speed regulating switch is switched to a designated position;
(5) installing a receiver;
(6) inputting a required temperature section, executing starting heating quantity, and properly adjusting voltage when the heating quantity is started;
(7) after distillation is finished, entering a cooling program to observe whether the cooling process is normal or not to check the effluent condition;
(8) when the temperature drops below 100 ℃, the instrument is turned off.
Preferably, the reduced pressure distillation in step a2 of the present invention specifically comprises the following steps:
(1) after a main power supply on a control cabinet of the heavy oil kettle type distillation instrument is turned on, a power supply switch of the instrument, and respective circulation switches and refrigeration switches are turned on;
(2) weighing the residual oil product after atmospheric distillation and the quality data of a distillation flask, connecting an experimental device, opening a stirring switch of a reduced pressure distillation kettle, and adjusting the stirring speed;
(3) checking whether the second receiver is aligned with the lifting column and the sampling needle tube, if not, aligning the second receiver, and aligning the second receiver with the lifting column and the sampling needle tube;
(4) during the setting, the name of the raw material, the weight of the kettle and the gross weight are sequentially input, the reduced pressure is selected, and the fraction number and the corresponding cutting temperature under the corresponding reduced pressure are set;
(5) heating, namely setting the heating amount to be 30% at first, adjusting the stirring until the liquid level just has vortex formation, then covering a heating cap, and inserting a power plug of the heating cap; the heating quantity is gradually increased along with the increase of the cutting temperature, so that the uniform flow rate is ensured;
(6) an operator is present to notice whether the running condition of the instrument is normal or not in the program executing process, and if a fault which cannot be timely eliminated occurs in the running process, a main power supply on the control cabinet is immediately turned off;
(7) when the products are temporarily cut or collected by the second receiver when the cutting temperature is reached, timely covering the cover of the second receiver after the turntable is turned, and attaching corresponding fraction labels to the cover of the second receiver;
(8) after distillation is finished, entering a cooling program to observe whether the cooling process is normal or not to check the effluent condition;
(9) when the temperature drops below 100 ℃, the instrument is closed;
(10) and (4) after the instrument is closed, pouring out residual oil in the vacuum distillation kettle while the residual oil is hot.
Preferably, the determination of the Engler viscosity of the residue to be measured in the step b1 of the invention specifically comprises the following steps:
(1) heating the residual oil to be tested to 110 ℃ of 100 ℃, and uniformly stirring;
(2) turning on a power supply of the Engler viscosity testing device, heating the outer container, opening the stirring rod, plugging the outflow hole of the viscometer when the liquid temperature of the outer container reaches 99.8-100.2 ℃, then injecting residual oil which is preheated to be slightly higher than a specified temperature into the inner container, wherein the oil level of the injected oil is higher than the tip of the spike; when the temperature of the thermometer in the residual oil sample to be measured reaches the specified temperature, keeping for 5min, lifting the wooden plug, starting the stopwatch at the same time, and reading the outflow time T1 of the sample when the sample in the receiving bottle reaches the marking line of 200 mL;
(3) simultaneously measuring the water value of the Engler viscometer, namely the time T2 required for the distilled water to flow out of 200mL from the viscometer at 20 ℃;
(4) the Engler viscosity of the residuum is calculated as follows:
E100=T1/T2
in the above formula:
e100- -residual oil Engler viscosity, Condition;
t1- -time required for sample to flow out of the viscometer for 200mL at test temperature 100 ℃, s;
t2- -water value, s of En viscometer.
Preferably, the chromatographic determination in step b2 of the present invention specifically comprises the following steps:
(1) after the Engler viscosity E100 of the residual oil at 100 ℃ is measured, if the E100 is less than or equal to 100, carbon tetrachloride is used for dissolving, if the E100 is more than 100, carbon disulfide is used for dissolving;
(2) heating and dissolving residual oil with the measured Engler viscosity, uniformly stirring, taking a sample bottle, weighing 0.3 g of sample and 2.0 g of carbon disulfide or carbon tetrachloride, recording specific numerical values, and covering a bottle cover in time;
(3) helium, hydrogen and air were turned on and the column temperature was raised to 40 ℃;
(4) putting the corresponding serial numbers of the sample bottles, opening a computer, editing the sequence and starting to run;
(5) after the sequence operation is completed, the distillation report and the quality yield report of each fraction of the residual oil are checked through a control chromatograph.
The invention has the beneficial effects that: the method comprises the steps of distilling crude oil at a real boiling point, heating and melting residual oil in a kettle after distillation, uniformly stirring, dissolving with carbon tetrachloride or carbon disulfide, analyzing by using a high-temperature simulated distillation liquid chromatography to obtain a distillation report and a quality yield report of the residual oil, obtaining the extractable rate of each fraction in the residual oil, checking the degree of coincidence with device data, determining the utilization efficiency of the crude oil, guiding process adjustment of oil refining production, product yield measurement and calculation, and economic benefit measurement and improvement of economic benefit.
Drawings
FIG. 1 is a schematic diagram of the real boiling point distiller of the present invention;
FIG. 2 is a schematic diagram of the heavy oil kettle still of the present invention;
FIG. 3 is a schematic view of an Engler viscosity testing apparatus of the present invention;
FIG. 4 is a schematic diagram of the high temperature simulated distillation apparatus of the present invention;
in the upper diagram: the system comprises a distillation kettle 1, a heating device 2, a distillation tower 3, a pressure display valve 4, a pressure difference controller 5, a receiver 6, a condenser pipe 7, a collector 8, a first vacuum pump 9, a second vacuum pump 10, a main cold water bath 11, a distillate water bath 12, a cold trap water bath 13 and a filter tower 14;
a reduced-pressure distillation kettle b2, a second heating device b1, a second distillation tower b3, a second pressure display valve b4, a second condensation pipe b5, a second collector b6, a second receiver b7, a second fraction water bath b8, a second cold trap water bath b9, a second pressure sensor b10, nitrogen b11, a vacuum pump b12, a gas trap b13, an emptying valve b14 and a vacuum sensor b 15;
inner container thermometer c1, stirring rod c2, outer container thermometer c3, inner container cover c4, inner container c5, outer container c6, cork c7, spike c8, heating rod c9, outflow hole c10, receiving bottle c11, temperature adjusting button c12, power switch c13, horizontal adjusting screw c14, instrument body c15 and bracket c 16;
chromatograph d1, sample bottle d2, sample injector d3 and computer d 4.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
The invention provides a method for measuring the extractable rate of each fraction of residual oil in crude oil, which comprises the following steps:
a. subjecting the crude oil to true boiling point distillation:
a1, atmospheric distillation: with reference to the attached FIG. 1
1, weighing a sample: record the empty retort mass of 2973.1g and the total weight of oil and retort weighed of 9189.2g
2 after the sample is weighed, placing the distillation kettle 1 on a heating device 2, adjusting the position to enable the distillation kettle 1 to be tightly connected with a distillation tower 3, then connecting a pressure display valve 4, connecting a water-cooling cooler 5, and clamping by a clamp to enable the contact part to be more sealed;
3 starting the computer connecting instrument to check whether the instrument is normally connected;
4, turning on a stirring switch by the heating sleeve, turning on a designated switch, and regulating the rotating speed;
5, installing a receiver 6;
6 setting the required temperature section at 0-160 ℃ under normal pressure, the required temperature section at 160-360 ℃ under 10torr pressure, and clicking to execute starting heating quantity (the voltage is properly adjusted when the heating quantity is started);
7, after the distillation is finished, entering a cooling program to observe whether the cooling process is normal or not to check the effluent condition;
8 when the temperature is reduced to be below 100 ℃, closing the instrument;
a2 distillation under reduced pressure, see FIG. 2
1, after a main power supply on a heavy oil kettle type distillation instrument control cabinet is turned on, turning on an instrument power supply switch and respective circulation switches and refrigeration switches;
2 weighing 1461.5g of the mass of the reduced pressure distillation kettle b2, 4573g of the total weight of the residual oil product after atmospheric distillation and the reduced pressure distillation kettle b2, connecting an experimental device, opening a stirring switch of the reduced pressure distillation kettle b2 and adjusting the stirring speed;
3 checking whether the second receiver b7 is aligned with the lifting column and the sampling needle tube, and if not, aligning the second receiver b 7;
4, inputting the name of the raw material, the weight of the kettle and the gross weight in sequence, selecting the decompression pressure of 0.2torr, and setting the cutting temperature at the corresponding decompression pressure of 160-;
5, starting heating, namely setting the heating quantity to be 30%, adjusting the stirring in the reduced pressure distillation kettle b2 until the liquid level is just formed with vortex, and then covering a heating cap and inserting a power plug of the heating cap; the heating quantity is gradually increased along with the increase of the cutting temperature, so that the uniform flow rate is ensured;
6, in the instrument execution process, an operator needs to pay attention to whether the instrument operation condition is normal or not in the field, and if a fault which cannot be timely eliminated occurs in the operation process, a main power supply on the control cabinet is immediately turned off;
7 when the products are collected in the second receiver b7 when the temporary cutting occurs or the cutting temperature is reached, timely covering the receiving pipe cover after the turntable is indexed, and attaching the corresponding fraction label on the second receiver b7 cover;
8, after the distillation is finished, entering a cooling program to observe whether the cooling process is normal or not to check the effluent condition;
9 when the temperature is reduced to be below 100 ℃, closing the power supply of the heavy oil kettle type distillation instrument;
10, turning off the instrument, and pouring out residual oil in the reaction kettle while the instrument is hot;
b. subjecting the residue remaining after completion of distillation to high temperature simulated distillation with reference to FIG. 3
b1, determination of the Engler viscosity of the to-be-detected residual oil:
1 heating the residual oil to be tested to 110 ℃ of 100 ℃ and uniformly stirring;
2, opening a power switch c13 of the Engler viscosity testing device, heating, opening a stirring rod c2, when the liquid temperature of the outer container c6 reaches 99.8-100.2 ℃, tightly plugging a flow-out hole c10 of the viscometer by using a wooden plug c7, then injecting residual oil which is preheated to be slightly higher than a specified temperature into an inner container c5, wherein the oil level of the injected residual oil is slightly higher than the tip of a sharp nail c 8; when the temperature c1 of the inner container in the residual oil sample to be detected just reaches the specified temperature, keeping for 5min, quickly lifting the wooden plug c7, simultaneously starting a stopwatch, and reading the outflow time T1 of the sample when the sample in the receiving bottle c11 just reaches the 200mL mark line;
3, simultaneously measuring the water value of the Engler viscometer, namely the time T2 required for the distilled water to flow out of 200mL from the viscometer at the temperature of 20 ℃;
4 the Engler viscosity of the residue was calculated as follows:
E100=T1/T2
in the formula:
e100- -residual oil Engler viscosity, Condition;
t1- -time required for sample to flow out of the viscometer for 200mL at test temperature 100 ℃, s;
t2- -water number, s, of En viscometer;
b2, chromatography, see FIG. 4,
1, measuring the Engler viscosity (E100) of the residual oil at 100 ℃ to be 95.61 conditional degrees, and dissolving the residual oil by using carbon disulfide;
2 opening the high-temperature simulated distillation apparatus: opening helium, hydrogen and air, and turning on a power supply of a chromatograph until the temperature of the column rises to 40 ℃;
3 heating and dissolving the residual oil with the measured Engler viscosity, uniformly stirring, taking a sample bottle, weighing 0.3011 g of sample and 2.1421 g of carbon disulfide, and timely covering a bottle cap (the solvent is volatile);
4, putting the sample bottles on a chromatograph in correspondence with the serial numbers, opening a computer, editing the sequence, inputting the serial numbers, the method names, the sample types, the sample qualities and the solvent qualities
And 5, after the sequence operation is finished, checking a distillation report and a quality yield report of each fraction of the residual oil by selecting a spectrogram through a computer-controlled chromatograph, and determining the extractable rate of each fraction.
TABLE-yield of each fraction of residue after true boiling point distillation
Referring to the attached figure 1, the atmospheric distillation device, also called as a true boiling point distillation apparatus, comprises a distillation still 1, a heating device 2, a distillation tower 3, a pressure display valve 4, a pressure difference controller 5, a receiver 6, a condenser pipe 7, a collector 8, a first vacuum pump 9, a second vacuum pump 10, a main cold water bath 11, a distillate water bath 12, a cold trap water bath 13 and a filter tower 14, wherein the main cold water bath 11 is arranged on one side of the heating device 2, the receiver 6 is arranged on the other side of the heating device, and the distillate water bath 12 and the cold trap water bath 13 are arranged on the right side of the receiver 6; a distillation kettle 1 is arranged at the upper part of the heating device 2, a distillation tower 3 is arranged above the distillation kettle 1, one side of the distillation kettle 1 is connected with a pressure display valve 4 and a pressure difference controller 5, a filter tower 14 is arranged at the upper part of the distillation tower 3, and the top of the filter tower is connected with a second vacuum pump 10 through a valve; the middle part of the distillation tower 3 is connected with a collector 8 through a condensing pipe 7, and a receiver 6 is arranged below the collector 8; and the collector 8 is connected with a first vacuum pump 9 through a pipeline.
Referring to fig. 2, the heavy oil kettle type distiller of the present invention is applied to vacuum distillation, and specifically includes a vacuum distillation kettle b2, a second heating device b1, a second distillation tower b3, a second pressure indicating valve b4, a second condensing pipe b5, a second collector b6, a second receiver b7, a second fraction water bath b8, a second cold trap water bath b9, a second pressure sensor b10, nitrogen b11, a vacuum pump b12, a gas trap b13, an emptying valve b14, and a vacuum sensor b15, wherein the vacuum distillation kettle b1 is installed at an upper portion of the second heating device b1, the second distillation tower b1 is installed at an upper portion of the vacuum distillation kettle b1, the second pressure indicating valve b1 is connected to one side of the vacuum distillation kettle b1, the second distillation tower b1 is connected to the second collector b1 through the second condensing pipe b1, the second receiver b1 is installed below the second collector b1, and the second receiver b1 is provided with the second fraction water bath 1, Second cold trap water bath b 9.
A pipeline is connected above the second receiver b7, one end of the pipeline is connected with a vacuum sensor b15, the other end of the pipeline is provided with an emptying valve b14, the left side of the emptying valve b14 is connected with a vacuum pump b12 through a gas trap b13, the left side of the gas trap b13 is connected with nitrogen b11 through a pipeline, and the pipeline is provided with a second pressure sensor b 10.
Referring to fig. 3, the present invention provides an emn viscosity testing device, comprising an inner container thermometer c1, a stirring rod c2, an outer container thermometer c3, an inner container cover c4, an inner container c5, an outer container c6, a cork c7, a spike c8, a heating rod c9, an outflow hole c10, a receiving bottle c11, a temperature adjusting button c12, a power switch c13, a horizontal adjusting screw c14, an instrument body c15, a bracket 16, wherein the inner cavity of the instrument body c15 is provided with the bracket c16, the upper side of the bracket c16 is provided with the outer container c6, the bottom of the outer container c6 is provided with the heating rod c9, the inner container c5 is provided with the inner cavity of the outer container c6, the bottom of the inner container c5 is provided with the outflow hole c10, the outflow hole c10 corresponds to the receiving bottle c11 below the bracket through the bottom of the outer container c6, and the outflow hole c10 is opened by the cork c 7; an inner container cover c4 is arranged on the top of the inner container c5, an inner container thermometer c1 and a wooden plug c7 are respectively inserted on the inner container cover c4, and an outer container thermometer c3 and a stirring rod c2 are arranged between the inner container c5 and the outer container c 6.
A plurality of sharp nails c8 are arranged in the middle of the inner cavity of the inner container c5, the outer wall of the receiving bottle c11 is marked with scales of 100ml and 200ml, the bottom of the instrument main body c15 is provided with a horizontal adjusting screw c14, and the outer wall of the lower side of the instrument main body c15 is provided with a temperature adjusting button c12 and a power switch c 13.
Referring to fig. 4, the high temperature simulated distillation apparatus of the present invention comprises a chromatograph d1, a sample bottle d2, a sample injector d3 and a computer d4, wherein the sample bottle d2 and the sample injector d3 are arranged on the upper part of the chromatograph d1, and the computer d4 is arranged on one side of the chromatograph d 1.
The above description is only a few of the preferred embodiments of the present invention, and any person skilled in the art may modify the above-described embodiments or modify them into equivalent ones. Therefore, any simple modifications or equivalent substitutions made in accordance with the technical solution of the present invention are within the scope of the claims of the present invention.
Claims (1)
1. A method for measuring the extractable rate of each fraction of residual oil in crude oil is characterized by comprising the following steps: the method comprises the following steps:
a. subjecting the crude oil to true boiling point distillation:
a1, atmospheric distillation:
1, weighing a sample and recording the total amount before weighing and the weight after weighing;
2, carrying out normal pressure distillation;
3 when the temperature is reduced to below 100 ℃, closing the instrument;
a2, vacuum distillation
1 weighing the residual oil product after atmospheric distillation and the quality data of a distillation flask, and starting reduced pressure distillation;
2 when the temperature is reduced to below 100 ℃, closing the instrument;
3, pouring out residual oil in the reaction kettle when the instrument is hot after the instrument is closed;
b. the residual oil left after distillation is subjected to high-temperature simulated distillation
b1, determination of Engler viscosity of residual oil to be measured
Heating and melting to-be-detected residual oil, uniformly stirring, measuring the Engler viscosity E100 at 100 ℃, and dissolving with carbon tetrachloride if the E100 is less than or equal to 100, or dissolving with carbon disulfide if the E100 is greater than 100;
b2, chromatography
1 heating and dissolving residual oil with measured Engler viscosity, uniformly stirring, taking a sample bottle, weighing 0.3 g of sample and 2.0 g of carbon disulfide or carbon tetrachloride, recording specific numerical values, and covering a bottle cover in time;
2, putting the corresponding serial numbers of the sample bottles, opening a computer, editing the sequence and starting to run;
3, after the sequence operation is finished, checking a distillation report and a quality yield report of each fraction of the residual oil by controlling a chromatograph;
the atmospheric distillation in the step a1 specifically comprises the following steps:
(1) weighing the sample and recording the total amount before weighing and the weight after weighing;
(2) after the sample is weighed, the distillation kettle is placed on a heating device, the position is adjusted to enable the distillation kettle to be tightly connected with the distillation tower, then a pressure display valve is connected, a water-cooling cooler is connected, and a clamp is used for clamping to enable the contact part to be more sealed;
(3) starting the computer, and connecting an instrument to check whether the instrument is normally connected;
(4) the upper heating sleeve turns on the stirring switch to turn on the designated switch, and the speed regulating switch is switched to a designated position;
(5) installing a receiver;
(6) inputting a required temperature section, executing starting heating quantity, and properly adjusting voltage when the heating quantity is started;
(7) after distillation is finished, entering a cooling program to observe whether the cooling process is normal or not to check the effluent condition;
(8) when the temperature drops below 100 ℃, the instrument is closed;
the reduced pressure distillation in the step a2 specifically comprises the following steps:
(1) after a main power supply on a control cabinet of the heavy oil kettle type distillation instrument is turned on, a power supply switch of the instrument, and respective circulation switches and refrigeration switches are turned on;
(2) weighing the residual oil product after atmospheric distillation and the quality data of a distillation flask, connecting an experimental device, opening a stirring switch of a reduced pressure distillation kettle, and adjusting the stirring speed;
(3) checking whether the second receiver is aligned with the lifting column and the sampling needle tube, if not, aligning the second receiver, and aligning the second receiver with the lifting column and the sampling needle tube;
(4) during the setting, the name of the raw material, the weight of the kettle and the gross weight are sequentially input, the reduced pressure is selected, and the fraction number and the corresponding cutting temperature under the corresponding reduced pressure are set;
(5) heating, namely setting the heating amount to be 30% at first, adjusting the stirring until the liquid level just has vortex formation, then covering a heating cap, and inserting a power plug of the heating cap; the heating quantity is gradually increased along with the increase of the cutting temperature, so that the uniform flow rate is ensured;
(6) an operator is present to notice whether the running condition of the instrument is normal or not in the program executing process, and if a fault which cannot be timely eliminated occurs in the running process, a main power supply on the control cabinet is immediately turned off;
(7) when the products are temporarily cut or collected by the second receiver when the cutting temperature is reached, timely covering the cover of the second receiver after the turntable is turned, and attaching corresponding fraction labels to the cover of the second receiver;
(8) after distillation is finished, entering a cooling program to observe whether the cooling process is normal or not to check the effluent condition;
(9) when the temperature drops below 100 ℃, the instrument is closed;
(10) after the instrument is closed, pouring out residual oil in the vacuum distillation kettle while the instrument is hot;
the determination of the Engler viscosity of the residual oil to be determined in the step b1 specifically comprises the following steps:
(1) heating the residual oil to be tested to 110 ℃ of 100 ℃, and uniformly stirring;
(2) turning on a power supply of the Engler viscosity testing device, heating the outer container, opening the stirring rod, plugging the outflow hole of the viscometer when the liquid temperature of the outer container reaches 99.8-100.2 ℃, then injecting residual oil which is preheated to be slightly higher than a specified temperature into the inner container, wherein the oil level of the injected oil is higher than the tip of the spike; when the temperature of the thermometer in the residual oil sample to be measured reaches the specified temperature, keeping for 5min, lifting the wooden plug, starting the stopwatch at the same time, and reading the outflow time T1 of the sample when the sample in the receiving bottle reaches the marking line of 200 mL;
(3) simultaneously measuring the water value of the Engler viscometer, namely the time T2 required for the distilled water to flow out of 200mL from the viscometer at 20 ℃;
(4) the Engler viscosity of the residuum is calculated as follows:
E100=T1/T2
in the above formula:
e100- -residual oil Engler viscosity, Condition;
t1- -time required for sample to flow out of the viscometer for 200mL at test temperature 100 ℃, s;
t2- -water number, s, of En viscometer;
the chromatographic determination in the step b2 specifically comprises the following steps:
(1) after the Engler viscosity E100 of the residual oil at 100 ℃ is measured, if the E100 is less than or equal to 100, carbon tetrachloride is used for dissolving, if the E100 is more than 100, carbon disulfide is used for dissolving;
(2) heating and dissolving residual oil with the measured Engler viscosity, uniformly stirring, taking a sample bottle, weighing 0.3 g of sample and 2.0 g of carbon disulfide or carbon tetrachloride, recording specific numerical values, and covering a bottle cover in time;
(3) helium, hydrogen and air were turned on and the column temperature was raised to 40 ℃;
(4) putting the corresponding serial numbers of the sample bottles, opening a computer, editing the sequence and starting to run;
(5) after the sequence operation is finished, checking a distillation report and a quality yield report of each fraction of the residual oil by controlling a chromatograph;
the atmospheric distillation device comprises a distillation kettle (1), a heating device (2), a distillation tower (3), a pressure display valve (4), a pressure difference controller (5), a receiver (6), a condensing pipe (7), a collector (8), a first vacuum pump (9), a second vacuum pump (10), a main cold water bath (11), a fraction water bath (12), a cold trap water bath (13) and a filter tower (14), wherein the main cold water bath (11) is arranged on one side of the heating device (2), the receiver (6) is arranged on the other side of the heating device, and the fraction water bath (12) and the cold trap water bath (13) are arranged on the right side of the receiver (6); a distillation kettle (1) is arranged at the upper part of the heating device (2), a distillation tower (3) is arranged above the distillation kettle (1), one side of the distillation kettle (1) is connected with a pressure display valve (4) and a pressure difference controller (5), a filter tower (14) is arranged at the upper part of the distillation tower (3), and the top of the filter tower is connected with a second vacuum pump (10) through a valve; the middle part of the distillation tower (3) is connected with a collector (8) through a condensing pipe (7), and a receiver (6) is arranged below the collector (8); the collector (8) is connected with a first vacuum pump (9) through a pipeline;
wherein, the heavy oil kettle type distiller is applied to reduced pressure distillation and comprises a reduced pressure distillation kettle (b 2), a second heating device (b 1), a second distillation tower (b 3), a second pressure display valve (b 4), a second condensing pipe (b 5), a second collector (b 6), a second receiver (b 7), a second fraction water bath (b 8), a second cold trap water bath (b 9), a second pressure sensor (b 10), nitrogen (b 11), a vacuum pump (b 12), a gas trap (b 13), a blow-down valve (b 14) and a vacuum sensor (b 15), the upper part of the second heating device (b 1) is provided with the reduced pressure distillation kettle (b 2), the upper part of the reduced pressure distillation kettle (b 2) is provided with the second distillation tower (b 3), one side of the reduced pressure distillation kettle (b 2) is connected with the second pressure display valve (b 4), and the distillation tower (b 3) is connected with the second collector (b 6) through the second condensing pipe (b 5), a second receiver (b 7) is arranged below the second collector (b 6), and a second distillate water bath (b 8) and a second cold trap water bath (b 9) are arranged on one side of the second receiver (b 7);
a pipeline is connected above the second receiver (b 7), one end of the pipeline is connected with a vacuum sensor (b 15), the other end of the pipeline is provided with an emptying valve (b 14), the left side of the emptying valve (b 14) is connected with a vacuum pump (b 12) through a gas trap (b 13), the left side of the gas trap (b 13) is connected with nitrogen (b 11) through a pipeline, and the pipeline is provided with a second pressure sensor (b 10);
the Engler viscosity testing device comprises an inner container thermometer (c 1), a stirring rod (c 2), an outer container thermometer (c 3), an inner container cover (c 4), an inner container (c 5), an outer container (c 6), a wooden plug (c 7), a spike (c 8), a heating rod (c 9), an outflow hole (c 10), a receiving bottle (c 11), a temperature adjusting button (c 12), a power switch (c 13), a horizontal adjusting screw (c 14), an instrument main body (c 15) and a bracket (c 16), wherein a bracket (c 16) is arranged in an inner cavity of the instrument main body (c 15), an outer container (c 6) is arranged on the upper side of the bracket (c 16), the heating rod (c 9) is arranged at the bottom of the outer container (c 6), the inner container (c 5) is arranged in the inner cavity of the outer container (c 6), an outflow hole (c 10) is arranged at the bottom of the inner container (539c 5), and the outflow hole (c 10) corresponds to the bottom of the receiving bottle (c 11) below the outer container (c 6), and the outflow hole (c 10) is closed and opened by the cooperation of a wooden plug (c 7); an inner container cover (c 4) is arranged at the top of the inner container (c 5), an inner container thermometer (c 1) and a wooden plug (c 7) are respectively inserted on the inner container cover (c 4), and an outer container thermometer (c 3) and a stirring rod (c 2) are arranged between the inner container (c 5) and the outer container (c 6);
a plurality of sharp nails (c 8) are arranged in the middle of the inner cavity of the inner container (c 5), the outer wall of the receiving bottle (c 11) is marked with scales of 100ml and 200ml, the bottom of the instrument main body (c 15) is provided with a horizontal adjusting screw (c 14), and the outer wall of the lower side of the instrument main body (c 15) is provided with a temperature adjusting button (c 12) and a power switch (c 13);
the instrument for high-temperature simulated distillation comprises a chromatograph (d 1), a sample bottle (d 2), a sample injector (d 3) and a computer (d 4), wherein the sample bottle (d 2) and the sample injector (d 3) are arranged on the upper part of the chromatograph (d 1), and the computer (d 4) is arranged on one side of the chromatograph (d 1).
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